CN104556594B - A kind of low temperature greasy filth emulsion splitter and preparation method thereof - Google Patents
A kind of low temperature greasy filth emulsion splitter and preparation method thereof Download PDFInfo
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- CN104556594B CN104556594B CN201310495653.7A CN201310495653A CN104556594B CN 104556594 B CN104556594 B CN 104556594B CN 201310495653 A CN201310495653 A CN 201310495653A CN 104556594 B CN104556594 B CN 104556594B
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- greasy filth
- emulsion splitter
- oil
- water
- filth emulsion
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
Abstract
The invention discloses a kind of low temperature greasy filth emulsion splitter and preparation method thereof, with emulsion splitter parts by weight, comprise following component: methyl glucamine 5 ~ 23 parts, fatty alcohol-polyoxyethylene ether 4 ~ 19 parts, 1 ~ 5 part, inorganic salt, 53 ~ 90 parts, water.Preparation method comprises following content: methyl glucamine, fatty alcohol-polyoxyethylene ether, inorganic salt and water are mixed, and obtains low temperature greasy filth emulsion splitter.This emulsion splitter low-temperature demulsification is effective, use temperature wide ranges, oil recovery rate are high, and have that production cost is low, the advantage such as environmental protection, preparation method are easy and have wide range of applications.Greasy filth emulsion splitter of the present invention can be applied to the harmless treatment of tank bottom oil sludge, scum silica frost and active sludge, also can be applied to the process of the various oily sludges of oil production and Transportation Enterprise generation.
Description
Technical field
The present invention relates to a kind of greasy filth emulsion splitter and preparation method thereof, particularly relate to a kind of low temperature greasy filth emulsion splitter and preparation method thereof.
Background technology
Oil exploitation, collect defeated, black solid, the semisolid waste of a large amount of oil-containing can be produced in refining and oily water treatment process, be referred to as greasy filth, its main component is oil, Ni Heshui.In greasy filth, solid particle size can from not enough micron to several inches, and great majority are between l to 100 micron, and crude oil kind, refinery structure and operational condition are depended in oil composition, and the composition of mud may change in time and change.According to statistics, nearly 3,000,000 tons of Chinese festiva produce oil mud, the crude resources wherein contained is about about 600,000 tons.Except containing except a large amount of aged crude oil, wax, colloidalmaterial in greasy filth, containing hazardous and noxious substances such as a large amount of benzene homologues, phenols, anthracene, pyrene, polychlorobiphenyl and Dioxins.In addition also contain a large amount of pathogenic bacterias, parasite in greasy filth, if do not carried out rationally effective process, not only can waste petroleum resources, also can cause severe contamination to environment.
The technology of current process oily sludge mainly contains resource reclaim, harmless treatment and comprehensive utilization technique etc.Resource reclaim treatment technology comprises solvent extration, WATER-WASHING METHOD, micro emulsion washing, breakdown of emulsion method etc.Greasy filth innoxious process for treating comprises immobilization process, the technology such as biological treatment, burning.Comprehensive utilization technique comprises thermolysis, brickmaking is paved the way and other purposes.The treatment technology of greasy filth is varied, and often kind of method has respective relative merits and the scope of application.
Have the advantages such as activity is high, instant effect due to chemical demulsifier, adding emulsion splitter is breaking method the most frequently used at present.The shortcomings such as it is low that emulsion splitter conventional at present mainly also exists oil recovery rate, low-temperature demulsification weak effect, biological degradability difference, and existing conventional emulsion splitter generally needs to carry out breakdown of emulsion at 70 DEG C ~ 90 DEG C.CN101050380A discloses a kind of base oildeemulsifier in high performance and preparation method thereof, and the composition principle of this emulsion splitter take W-Gum as starting raw material, introduces after conventional polyether type emulsion splitter carries out graft copolymerization and obtains.This emulsion splitter has the features such as service temperature gentleness, cost is low, demulsification is good, but preparation process is comparatively complicated, also needs to add protonic acid and organic solvent, is unfavorable for environmental protection, and concrete demulsification also lacks the support of related data.CN102039301A discloses a kind of oily sludge resource utilization, Harmless and Comprehensive Disposal technique.Emulsion splitter wherein used is two or more mixture in sodium carbonate, sodium sulfate, sodium laurylsulfonate, polyoxyethylene lauryl ether, and oil recovery rate can reach 75% ~ 90%.This technological process is comparatively complicated, and oil recovery rate needs to improve.CN102492460A discloses a kind of crude oil low-temperature demulsifier preparation method and application, the method prepares emulsion splitter by polyethylene polyamine polyethers and alkyl phenol polyether, this emulsion splitter has breaking emulsion and dewatering speed faster at 34 ~ 38 DEG C at a lower temperature, dehydration rate reaches more than 90%, but undesirable to the process of the high oily sludge of solid content, also lack the related data of concrete oil recovery rate.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of low temperature greasy filth emulsion splitter and preparation method thereof.This emulsion splitter low-temperature demulsification is effective, oil recovery rate is high, and production cost is low, environmental protection, preparation method are simple and applied range.
Low temperature greasy filth emulsion splitter of the present invention, with emulsion splitter parts by weight, comprises following component:
Methyl glucamine 5 ~ 23 parts
Fatty alcohol-polyoxyethylene ether 4 ~ 19 parts
1 ~ 5 part, inorganic salt
53 ~ 90 parts, water
The molecular formula of methyl glucamine of the present invention (MEGA) is R-C
8h
16o
6n, wherein R is C
8~ C
18alkyl.
The molecular formula of fatty alcohol-polyoxyethylene ether of the present invention (AEO) is R-O (CH
2cH
2o)
nh, wherein R is C
12~ C
18alkyl, n=6 ~ 20.
Inorganic salt of the present invention are one or more in sodium-chlor, Repone K, sodium sulfate or potassium sulfate.
The present invention can add inhibiter as required, and as one or more in type oxide film inhibiter, deposition membranous type inhibiter or adsorbed film type inhibiter, the add-on of inhibiter according to actual needs, generally accounts for 0.1% ~ 1% of greasy filth emulsion splitter weight.
The present invention can add sequestrant as required, and as one or more in citric acid, 4A zeolite or gluconate, the add-on of sequestrant according to actual needs, generally accounts for 0.1% ~ 0.5% of greasy filth emulsion splitter weight.
The preparation method of low temperature greasy filth emulsion splitter of the present invention, comprises following content: methyl glucamine, fatty alcohol-polyoxyethylene ether, inorganic salt and water are mixed, and obtains low temperature greasy filth emulsion splitter of the present invention.Wherein, mixing time is 20 ~ 70 minutes, and mixing temperature is 10 ~ 40 DEG C.
Greasy filth emulsion splitter of the present invention can be applied to the harmless treatment of tank bottom oil sludge, scum silica frost and active sludge, and also can be applied to the process of the various oily sludges of oil production and the generation of storing enterprise, the greasy filth high to oil length is particularly applicable.
The detailed process that greasy filth emulsion splitter of the present invention is applied to oil-sludge treatment is as follows: first mixed in mixing tank with water by greasy filth, then greasy filth emulsion splitter is added, stir, the product after breakdown of emulsion carries out the three phase separation of oil, water, mud in oil-sludge separation device.
Wherein, the mass ratio of greasy filth and water is 1:3 ~ 1:8, and the mass percent that greasy filth emulsion splitter add-on accounts for greasy filth is 3% ~ 10%, and breakdown of emulsion temperature is 30 ~ 80 DEG C, and churning time is 20 ~ 120 minutes.
A kind of nonionogenic tenside that the methyl glucamine that greasy filth emulsion splitter of the present invention adopts is is Material synthesis with the renewable resources such as vegetables oil and starch.Methyl glucamine is nontoxic, little to skin irritation, and biological degradability can reach 98% ~ 99%; Performance is gentle, and is not easily acted upon by temperature changes; Good with the compatibleness of other tensio-active agents; To environment and biological safety high, environmental protection.Described fatty alcohol-polyoxyethylene ether is environmental protection tensio-active agent, has good biodegradability and low-temperature stability.Methyl glucamine and the composite use of fatty alcohol-polyoxyethylene ether, there is higher breakdown of emulsion synergism, be specially adapted to oily sludge and carry out breakdown of emulsion reaction under cryogenic, overcome the hot conditions needed for the reaction of traditional oily sludge breakdown of emulsion, to oily sludge, there is good breakdown of emulsion characteristic, and the rate of recovery of oil product is high.
Emulsion splitter of the present invention compares with traditional emulsion splitter, has the following advantages:
(1) emulsion splitter low-temperature demulsification of the present invention is effective, and oil recovery rate is high;
(2) emulsion splitter biological degradability of the present invention is good, little on the impact of environment and biology, environmental protection;
(3) emulsion splitter temperature influence of the present invention is less, and stability is strong;
(4) emulsion splitter of the present invention is adding less, and production cost is low, and preparation method is easy, applied widely, is easy to industrial application.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated, but therefore do not limit the present invention.
Embodiment 1
By methyl glucamine (R=C
8) 4g, fatty alcohol-polyoxyethylene ether (R=C
13, n=7) and 17g, Repone K 1.5g, water 77.5g, mix 35 minutes at normal temperatures, obtain greasy filth emulsion splitter.
Embodiment 2
By methyl glucamine (R=C
12) 15g, fatty alcohol-polyoxyethylene ether (R=C
12, n=6) and 11g, sodium-chlor 1g, water 73g, mix 38 minutes at normal temperatures, obtain greasy filth emulsion splitter.
Embodiment 3
By methyl glucamine (R=C
10) 21g, fatty alcohol-polyoxyethylene ether (R=C
14, n=10) and 5g, sodium sulfate 1.2g, water 72.88g, mix 30 minutes at normal temperatures, obtain greasy filth emulsion splitter.
Embodiment 4
Certain refinery's tank bottom oil sludge character is as follows: oil-containing 68.76%, and moisture 5.29%, solid matter content is 25.95%(percentage composition take weight as benchmark).
Tank bottom oil sludge is sent by pumping in mixing tank, makes the solid-to-liquid ratio of greasy filth and water in tank be 1:6, through strong stirring 7 minutes, greasy filth is mixed with water.In mixing tank, add according to greasy filth weight 5% the greasy filth emulsion splitter that embodiment 2 obtains, temperature of reaction maintains 30 ~ 48 DEG C, churning time 35 minutes.The reacted product of breakdown of emulsion carries out the separation of oil, water, mud in oil-sludge separation device, by isolated for top recovery of oil, is undertaken settlement separate by the mixture of the mud of bottom and water.Final oil recovery rate is 97.9%.
Embodiment 5
Selected greasy filth is with embodiment 4.
Tank bottom oil sludge is sent by pumping in mixing tank, makes the solid-to-liquid ratio of greasy filth and water in tank be 1:6, through strong stirring 7 minutes, greasy filth is mixed with water.In mixing tank, add according to greasy filth weight 5% the greasy filth emulsion splitter that embodiment 2 obtains, temperature of reaction maintains 60 ~ 90 DEG C, churning time 35 minutes.The reacted product of breakdown of emulsion carries out the separation of oil, water, mud in oil-sludge separation device, by isolated for top recovery of oil, is undertaken settlement separate by the mixture of the mud of bottom and water.Final oil recovery rate is 97.8%.
Comparative example 1
Selected greasy filth is with embodiment 4.
Tank bottom oil sludge is sent by pumping in mixing tank, makes the solid-to-liquid ratio of greasy filth and water in tank be 1:6, through strong stirring 7 minutes, greasy filth is mixed with water.In mixing tank, add polyether type demulsifying agent SP169 according to greasy filth weight 5%, temperature of reaction maintains 30 ~ 48 DEG C, churning time 35 minutes.The reacted product of breakdown of emulsion carries out the separation of oil, water, mud in oil-sludge separation device, by isolated for top recovery of oil, is undertaken settlement separate by the mixture of the mud of bottom and water.Final oil recovery rate is 71.5%.
Comparative example 2
Selected greasy filth is with embodiment 4.
Tank bottom oil sludge is sent by pumping in mixing tank, makes the solid-to-liquid ratio of greasy filth and water in tank be 1:6, through strong stirring 7 minutes, greasy filth is mixed with water.In mixing tank, add polyether type demulsifying agent SP169 according to greasy filth weight 5%, temperature of reaction maintains 60 ~ 90 DEG C, churning time 35 minutes.The reacted product of breakdown of emulsion carries out the separation of oil, water, mud in oil-sludge separation device, by isolated for top recovery of oil, is undertaken settlement separate by the mixture of the mud of bottom and water.Final oil recovery rate is 82.7%.
Comparative example 3
Selected greasy filth is with embodiment 4.Just methyl glucamine (R=C
12) 15g, sodium-chlor 1g, water 84g, mix 38 minutes at normal temperatures, obtain greasy filth emulsion splitter A.
Tank bottom oil sludge is sent by pumping in mixing tank, makes the solid-to-liquid ratio of greasy filth and water in tank be 1:6, through strong stirring 7 minutes, greasy filth is mixed with water.In mixing tank, add greasy filth emulsion splitter A according to 5% of greasy filth weight, temperature of reaction maintains 30 ~ 48 DEG C, churning time 35 minutes.The reacted product of breakdown of emulsion carries out the separation of oil, water, mud in oil-sludge separation device, by isolated for top recovery of oil, is undertaken settlement separate by the mixture of the mud of bottom and water.Final oil recovery rate is 69.3%.
Comparative example 4
Selected greasy filth is with embodiment 4.By fatty alcohol-polyoxyethylene ether (R=C
12, n=6) and 15g, sodium-chlor 1g, water 84g, mix 38 minutes at normal temperatures, obtain greasy filth emulsion splitter B.
Tank bottom oil sludge is sent by pumping in mixing tank, makes the solid-to-liquid ratio of greasy filth and water in tank be 1:6, through strong stirring 7 minutes, greasy filth is mixed with water.In mixing tank, add greasy filth emulsion splitter B according to 5% of greasy filth weight, temperature of reaction maintains 30 ~ 48 DEG C, churning time 35 minutes.The reacted product of breakdown of emulsion carries out the separation of oil, water, mud in oil-sludge separation device, by isolated for top recovery of oil, is undertaken settlement separate by the mixture of the mud of bottom and water.Final oil recovery rate is 67.4%.
Comparative example 5
Selected greasy filth is with embodiment 4.
Tank bottom oil sludge is sent by pumping in mixing tank, makes the solid-to-liquid ratio of greasy filth and water in tank be 1:6, through strong stirring 7 minutes, greasy filth is mixed with water.In mixing tank, add greasy filth emulsion splitter A according to 5% of greasy filth weight, temperature of reaction maintains 60 ~ 90 DEG C, churning time 35 minutes.The reacted product of breakdown of emulsion carries out the separation of oil, water, mud in oil-sludge separation device, by isolated for top recovery of oil, is undertaken settlement separate by the mixture of the mud of bottom and water.Final oil recovery rate is 79.2%.
Comparative example 6
Selected greasy filth is with embodiment 4.
Tank bottom oil sludge is sent by pumping in mixing tank, makes the solid-to-liquid ratio of greasy filth and water in tank be 1:6, through strong stirring 7 minutes, greasy filth is mixed with water.In mixing tank, add greasy filth emulsion splitter B according to 5% of greasy filth weight, temperature of reaction maintains 60 ~ 90 DEG C, churning time 35 minutes.The reacted product of breakdown of emulsion carries out the separation of oil, water, mud in oil-sludge separation device, by isolated for top recovery of oil, is undertaken settlement separate by the mixture of the mud of bottom and water.Final oil recovery rate is 78.6%.
Claims (11)
1. a low temperature greasy filth emulsion splitter, is characterized in that: with emulsion splitter parts by weight, comprises following component:
Methyl glucamine 5 ~ 23 parts
Fatty alcohol-polyoxyethylene ether 4 ~ 19 parts
1 ~ 5 part, inorganic salt
53 ~ 90 parts, water; Described inorganic salt are one or more in sodium-chlor, Repone K, sodium sulfate or potassium sulfate.
2. according to greasy filth emulsion splitter according to claim 1, it is characterized in that: the molecular formula of methyl glucamine is R-C
8h
16o
6n, wherein R is C
8~ C
18alkyl.
3. according to greasy filth emulsion splitter according to claim 1, it is characterized in that: the molecular formula of fatty alcohol-polyoxyethylene ether is R-O (CH
2cH
2o)
nh, wherein R is C
12~ C
18alkyl, n=6 ~ 20.
4. according to greasy filth emulsion splitter according to claim 1, it is characterized in that: add one or more in type oxide film inhibiter, deposition membranous type inhibiter or adsorbed film type inhibiter in greasy filth emulsion splitter, the add-on of inhibiter accounts for 0.1% ~ 1% of greasy filth emulsion splitter weight.
5. according to greasy filth emulsion splitter according to claim 1, it is characterized in that: containing one or more in citric acid, 4A zeolite or gluconate in greasy filth emulsion splitter, add-on accounts for 0.1% ~ 0.5% of greasy filth emulsion splitter weight.
6. a preparation method for greasy filth emulsion splitter according to claim 1, is characterized in that comprising following content: methyl glucamine, fatty alcohol-polyoxyethylene ether, inorganic salt and water are mixed, and obtains low temperature greasy filth emulsion splitter.
7. in accordance with the method for claim 6, it is characterized in that: mixing time is 20 ~ 70 minutes, mixing temperature is 10 ~ 40 DEG C.
8. the application in the process of various oily sludges that produces in the harmless treatment of tank bottom oil sludge, scum silica frost and active sludge and oil production and storing enterprise of a greasy filth emulsion splitter according to claim 1.
9. according to application according to claim 8, it is characterized in that: the detailed process that greasy filth emulsion splitter is applied to oil-sludge treatment is as follows: first mixed in mixing tank with water by greasy filth, then greasy filth emulsion splitter is added, stir, the product after breakdown of emulsion carries out the three phase separation of oil, water, mud in oil-sludge separation device.
10. according to application according to claim 9, it is characterized in that: the mass ratio of greasy filth and water is 1:3 ~ 1:8, the mass percent that greasy filth emulsion splitter add-on accounts for greasy filth is 3% ~ 10%.
11., according to application according to claim 9, is characterized in that: breakdown of emulsion temperature is 30 ~ 80 DEG C, and churning time is 20 ~ 120 minutes.
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| CN106281408A (en) * | 2016-09-08 | 2017-01-04 | 合肥智慧殿投资管理有限公司 | A kind of viscous crude demulsifier and its preparation method and application |
| CN108585390A (en) * | 2017-03-16 | 2018-09-28 | 哈尔滨工业大学（威海） | A kind of self-stabilization micro-nano lotion and its application process in oily sludge separation |
| CN107216008A (en) * | 2017-08-04 | 2017-09-29 | 浙江绿垚生态环境有限公司 | The formula and preparation method of a kind of oily sludge demulsifier |
| CN107973506B (en) * | 2017-12-29 | 2020-11-10 | 山东省科学院生态研究所 | Demulsifier for conditioning and three-phase separation of oily sludge and preparation method thereof |
| CN108751632A (en) * | 2018-05-22 | 2018-11-06 | 四川深蓝环保科技有限公司 | A kind of processing system and method for oily sludge |
| CN108675577A (en) * | 2018-05-22 | 2018-10-19 | 四川深蓝环保科技有限公司 | A kind of processing method of oily sludge |
| CN109020107A (en) * | 2018-06-19 | 2018-12-18 | 辽宁兴望源环保科技有限公司 | Greasy filth demulsification three phase separation agent and its preparation process |
| CN109574423A (en) * | 2018-11-20 | 2019-04-05 | 重庆奥图亚模型有限公司 | A kind of high-efficiency oil sludge demulsifier and preparation method thereof |
| CN111285583A (en) * | 2020-02-18 | 2020-06-16 | 北京中能诺泰节能环保技术有限责任公司 | Oil sludge demulsifier and preparation method thereof |
| CN111960625A (en) * | 2020-08-19 | 2020-11-20 | 中国特种设备检测研究院 | Oil sludge demulsifier and preparation method thereof |
| CN111847817B (en) * | 2020-09-01 | 2022-11-11 | 广西大学 | Oil sludge demulsifier, preparation method and application thereof |
| CN114702977B (en) * | 2022-03-28 | 2024-03-19 | 江苏天鹏龙辉环境科技有限公司 | Method for treating difficult-to-treat oil sludge in petrochemical enterprise electric desalting tank |
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